Sodium Hydroxide → 2-(2,5-Difluorophenylthio)-5-chlorobenzaldehyde

HRID 1388535

반응식

HRID 1388535 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[SH:9].[OH-].[Na+].Cl[C:13]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:14]=1[CH:15]=[O:16]>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[S:9][C:13]1[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][C:14]=1[CH:15]=[O:16]

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 807022,5-DichlorobenzaldehydeHCID 38363232,5-Difluorobenzene-1-thiol

생성물 1

HCID 128159512-(2,5-Difluorophenylthio)-5-chlorobenzaldehyde수율 74%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

The solution of 13.1 g of 2,5-difluorothiophenol (I.Cervena et al., Collect. Czech. Chem. Commun. 45, 2688, 1980) in 20 ml hexamethylphosphortriamide is treated with a solution of 3.6 g of sodium hydroxide in 6 ml of water and then with 13.65 g of 2,5-dichlorobenzaldehyde (of Example 6, reference above). Then, the mixture is heated while stirring for 5.5 hours to 100° C. It is then diluted with 150 ml of water and extracted with benzene. The extract is washed with a 5% sodium hydroxide solution and water, dried with magnesium sulfate and evaporated. The residue is crystallized from a mixture of benzene and petroleum ether. There are obtained 16.4 g (74%) 2-(2,5-difluorophenylthio)-5-chlorobenzaldehyde which melts in a pure state at 88°-90° C.

후처리

  1. temperatureThen, the mixture is heated
  2. extractionextracted with benzene
  3. washThe extract is washed with a 5% sodium hydroxide solution and water
  4. dry with materialdried with magnesium sulfate
  5. customevaporated
  6. customThe residue is crystallized from a mixture of benzene and petroleum ether

출처 및 근거

ORD 기록
ord-6002b79d316e46049eaffc1415cdfd10
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04431808

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